双水相萃取法在白酒中氨基甲酸乙酯 检测中的应用
目的 建立了双水相萃取结合气相色谱质谱法(gas chromatography-mass spectrometry, GC/MS)测定不同香型白酒中氨基甲酸乙酯的测定方法。方法 对比研究了3种不同的样品液液萃取方法, 在此基础上, 优化获得了最优双水相萃取(LLE-GC/MS)方案: 准确移取5 mL试样于10 mL比色管中, 再加入内标PC使用液, 逐渐增加管中K2HPO4固体, 直到饱和为止, 静置至分层完全。取上清液1.5 mL于离心管中, 加无水MgSO4 150 mg摇匀离心。取上清直接进样, 用GC/MS检测样品中氨基甲酸乙酯的含量。通过分别检测白酒三大香型: 清香、浓香、酱香型, 对LLE-GC/MS方法进行了评价。结果 在最优条件下检测的相对标准偏差为2.84%~3.95%, 回收率为: 86.45%~111.58%, 检测限为1.34 μg/L。结论 此方法准确性好、简便、低成本, 适用于上述3种香型白酒中氨基甲酸乙酯的检测。
Objective To establish a novel method to detect ethyl carbamate in different kinds of flavor liquor by liquid/liquid extractions (LLE) with gas chromatography mass spectrometry (GC/MS). Methods The efficiencies of 3 kinds of liquid/liquid extraction(LLE) in the extraction of ethyl carbamate from liquor were compared, and the optimum conditions of detecting ethyl carbamate in liquor were obtained as follow: for LLE extraction, 5 mL sample were filled accurately in a 10-mL colorimetric tube spiked with PC as the internal standard, then solid K2HPO4 was added gradually until it saturated with K2HPO4 and standing until completely separated. Supernatant 1.5 mL was transferred to a new centrifuge tube with 150 mg of MgSO4, after shaking well and centrifugation, the acquired supernatant was directly injected into GC/MS. Moreover, the method of LLE-GC/MS was evaluated through determination of ethyl carbamate in Fen-flavor liquor, Luzhou-flavor liquor, and Maotai-liquor, respectively. Results At the optimum conditions of detecting ethyl carbamate, the relative standard deviation was 2.84%~3.95% and the average recovery was 86.45%~111.58%. Limit of detection was 1.34 μg/L. Conclusion This method is a simple, accurate and less cost method to determine ethyl carbamate in 3 kinds of different flavor liquor.
标题：双水相萃取法在白酒中氨基甲酸乙酯 检测中的应用
英文标题：Application of liquid/liquid extraction in determination of ethyl carbamate in liquor
作者：
李园子 工业微生物教育部重点实验室,天津市工业微生物重点实验室,天津科技大学生物工程学院
黄世永 工业微生物教育部重点实验室,天津市工业微生物重点实验室,天津科技大学生物工程学院
郭学武 工业微生物教育部重点实验室,天津市工业微生物重点实验室,天津科技大学生物工程学院
杜丽平 工业微生物教育部重点实验室,天津市工业微生物重点实验室,天津科技大学生物工程学院
陈叶福 工业微生物教育部重点实验室,天津市工业微生物重点实验室,天津科技大学生物工程学院
肖冬光 工业微生物教育部重点实验室,天津市工业微生物重点实验室,天津科技大学生物工程学院
中文关键词:氨基甲酸乙酯,双水相萃取,气相色谱-质谱法,白酒,
英文关键词:ethyl carbamate,liquid/liquid extraction,gas chromatography-mass spectrometry,liquor,
发表日期：2015-05-12
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